大环糖肽抗生素键合相高效液相色谱法拆分7种氨基带保护基的氨基酸对映体

采用高效液相色谱法在装有大环糖肽抗生素键合相的手性柱上拆分了7种氨基带有芴甲氧羰基(fluorenylmethoxycarbonyl,Fmoc)保护的氨基酸对映体。比较了Fmoc-缬氨酸和相应的不带保护基的缬氨酸对映体在不同流动相体系中的色谱保留行为；考察了甲醇-醋酸-三乙胺流动相体系中醋酸和三乙胺的浓度以及它们二者的浓度之比对N-Fmoc氨基酸对映体拆分效果的影响。实验结果表明分离温度及流动相流速的变化也会对分离结果产生影响。该法简便快速,已成功地用于这类氨基酸的光学纯度测定。

Separation of Enantiomers of Amino Acid Derivatives by High Performance Liquid Chromatography on Teicoplanin Chiral Stationary Phase

Direct enantioseparations of seven N-fluorenylmethoxycarbonyl-amino acids (Fmoc-Val, Fmoc-Ser, Fmoc-Leu, Fmoc-Ile, Fmoc-Met, Fmoc-Ala, and Fmoc-Phe) were achieved by high performance liquid chromatography using a 250 mm x 4. 6 mm i.d. column bonded teicoplanin on silica gel as chiral stationary phase and methanol-acetic acid-triethylamine mixtures as mobile phase. The comparison of retention behavior and enantioseparation of N-Fmoc-Val and its non-blocked analogue on a Chirobiotic column with different mobile phase systems is presented. The effects of the content of acetic acid and triethylamine and the content ratio of acetic acid and triethylamine in the mobile phase on the enantioseparation of some N-Fmoc-amino acids were examined. The results showed that variations of column temperatureand flow rate of mobile phase also had effects on enantioseparation of N-Fmoc-amino acids. The method had been successfully applied to the determination of optical purity of some derivatized amino acids.